تفاعل #1914812

ord-c275d2d2912d488dbea11a462a090235

معادلة التفاعل

NNc1ccccn1
2-hydrazinopyridine
CCOC=CC#N
3-ethoxyacrylonitrile
NNc1ccccn1
2-Hydrazinopyridine
Nc1ccnn1-c1ccccn1
2-pyridin-2-yl-2H-pyrazol-3-ylamine

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةto reflux for 5 h
  2. 2
    درجة الحرارةto reflux for 4 h
  3. 3
    تركيزthe mixture is concentrated under reduced pressure until the excess hydrazinopyridine
  4. 4
    أخرىhas precipitated
  5. 5
    أخرىThe filtrate was purified by column chromatography

الإجراء التجريبي

A solution of 2-hydrazinopyridine (38.9 g, 453 mmol) was slowly added to a solution of 3-ethoxyacrylonitrile (31.5 g, 324 mmol) in pentanol (155 ml). The reaction mixture was brought to reflux for 5 h. 2-Hydrazinopyridine (10.6 g, 97 mmol) was again added and the reaction was allowed to continue to reflux for 4 h. The progress of the reaction is observed by TLC and, when the reaction is complete, the mixture is concentrated under reduced pressure until the excess hydrazinopyridine has precipitated. The filtrate was purified by column chromatography to give 2-pyridin-2-yl-2H-pyrazol-3-ylamine in the form of a white solid (2.75 g, 5.3%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07056354B2uspto-grants-2006_06